C22H20BrN3NiO5, triclinic, P1 (no. 2), a = 7.5761(8) A, b = 12.030(1) A, c = 13.255(1) A, 0 = 105.873(2)°, . = 97.984(2)°, = 95.002(2)°, V = 1140.8 A, Z = 2, Rgt(F) = 0.040, wRref(F) = 0.108, T = 293 K. Source of material The Schiff base ligand was synthesized by condensation 5bromo-2,3-diaminopyridine and 2-hydroxy-3-methoxybenzaldehyde with the ratio 1 : 2 in ethanol. The synthesis of the title complex was carried out by reacting Ni(ClO4)2 · 6H2O and the schiff base ligand (1:1, molar ratio) in methanol. After stirring, the process was continued for about 30 min at room temperature. The mixture was filtered and the filtrate was allowed to partially evaporate in air for sevral days to produce red-brown crystals suitable for X-ray diffraction with a yield about 60 %. Discussion Schiff-bases have played an important role in the development of coordination chemistry as they readily form stable complexes withmost of the transitionmetals, inwhich some could exhibit interesting properties [1-4]. The coordination sphere for theNi(II) ion in the title crystal structure is a slightly distorted square planar, in which the four positions are occupied by twoN atoms and twoO atoms of the Schiffbase ligand. The mean deviation from the plane formed by the two N atoms, two O atoms and the Ni ion is only 0.035A, indicative of that these five atoms can form a perfect plane. The bond lengths of Ni—N are 1.874(3) A and 1.929(3) A, and Ni—O 1.861(2) A and 1.905(2) A, respectively, are consistant with the corresponding distances in 6,6'-dimethoxy-2,2'-(ethane-1,2-diyl-bis(nitrilomethylidyne)diphenolato)nickel(II) [5]. Z. Kristallogr. NCS 224 (2009) 311-312 / DOI 10.1524/ncrs.2009.0138 311 © by Oldenbourg Wissenschaftsverlag, Munchen Crystal: red-brown block, size 0.19 × 0.21 × 0.23 mm Wavelength: Mo K0 radiation (0.71073 A) &: 26.40 cm−1 Diffractometer, scan mode: Bruker APEX II CCD, +/1 2max: 50.02° N(hkl)measured, N(hkl)unique: 5614, 3964 Criterion for Iobs, N(hkl)gt: Iobs > 2 !(Iobs), 3017 N(param)refined: 293 Programs: SHELXS-97 [6], SHELXL-97 [7], XP [8] Table 1. Data collection and handling. H(5) 2i 0.3038 0.8057 0.2390 0.106 H(3) 2i 0.3084 1.2634 0.7394 0.059 H(5A) 2i 0.1176 1.5086 0.6106 0.062 H(9) 2i 0.4536 0.6113 0.5403 0.063 H(10) 2i 0.5600 0.7455 0.7080 0.067 H(11) 2i 0.5148 0.9380 0.7396 0.061 H(12) 2i 0.3823 1.0900 0.6809 0.049 H(13A) 2i 0.4226 0.5243 0.3467 0.095 H(13B) 2i 0.2396 0.4897 0.2673 0.095 H(13C) 2i 0.2443 0.4948 0.3871 0.095 H(17) 2i −0.3004 0.8838 −0.0654 0.072 H(18) 2i −0.3192 1.0831 −0.0358 0.073 H(19) 2i −0.1992 1.2121 0.1278 0.066 H(20A) 2i −0.3411 0.6953 −0.0436 0.145 H(20B) 2i −0.1850 0.6200 −0.0318 0.145 H(20C) 2i −0.1643 0.7183 −0.0878 0.145 H(21) 2i −0.0372 1.2550 0.3111 0.052 H(22A) 2i 0.2666 0.7021 0.0428 0.137 H(22B) 2i 0.1772 0.6601 0.1281 0.137 H(22C) 2i 0.3726 0.6349 0.1122 0.137 Table 2. Atomic coordinates and displacement parameters (in A). Atom Site x y z Uiso